US9415442B2ActiveUtilityA1

Stable oxide encapsulated metal clusters and nanoparticles

Individually held — no corporate assignee on recordPriority: Apr 11, 2011Filed: Apr 11, 2012Granted: Aug 16, 2016
Est. expiryApr 11, 2031(~4.7 yrs left)· nominal 20-yr term from priority
B22F 1/16B22F 1/054C22C 5/06C22C 5/04B01J 23/42B82Y 30/00Y10S977/92C22C 5/02C09K 11/87C09K 11/025Y10S977/81Y10S977/89B01J 23/44C09K 11/58B82Y 5/00G01N 33/587B01J 23/52B22F 9/24B22F 1/02B22F 1/0018
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Claims

Abstract

The present invention discloses stable, non-agglomerated, ultra-small metal/alloy clusters encapsulated in silica with the metal/alloy cluster size of less than 5 nm. The invention further discloses a simple, cost effective process for the preparation of metal/alloy clusters encapsulated in silica which is thermally stable and without agglomeration.

Claims

exact text as granted — not AI-modified
We claim: 
     
       1. A process for synthesis of stable, non-agglomerated ultra-small clusters of metals/alloy having size less than 5 nm encapsulated in mono-disperse silica particles comprising;
 a. obtaining metal/alloy-thiolate clusters of less than 2 nm by modified Brust method using a 3:1 ratio of metal/alloy:thiol in a 1:1 mixture of methanol and water, using thiolate ligand N, N, N-Tripropyl (11-mercaptoundecyl) ammonium Chloride; 
 b. encapsulating with silica by a one step hydrolysis using tetraethyl orthosilicate (TEOS) in ethanol-water mixture to obtain monodisperse silica spheres encapsulating the metal/alloy clusters having a size less than 2 nm, and 
 c. further comprising calcining the monodisperse silica particles encapsulating the ultra-small metal/alloy clusters under a flow of air at 350° C., to obtain stable metal/alloy clusters with a nanoparticle size of less than 5 nm. 
 
     
     
       2. The process for the encapsulation according to  claim 1 , wherein the ultra-small clusters of metal/alloy are encapsulated in mono disperse silica particles of 20-30 nm diameter.

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